Process of hydrogenating carbon compounds under high pressure and elevated temperature



F. BERGIUS.

PROCESS OF HYDROGENATING CARBON COMPOUNDS UNDER HIGH PRESSURE AND'ELEVATED TEMPERATURE.

APPLICATION FILED APR. 18. I916.

1,391 364. Pammdse t. 27,1921;

prounds Under Hlgh UNITED sfr'afrss- PATENT-l osrrcs.

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To all whom it may concern:

Be it known that I, Dr. Fnmnmc'rr BER- oIUs, a citizen of the 'Empire ofGermany, residing at Iilssen-Ruhr, Germany, have 1n- 5- vented certainnew and useful Improvements in Processes of Hydrogenating CarbonComressure and Elevated emperature, (for whichI'have filed ap 110ationsin'German on Dec-'24, 1914, an July 17, 1915,) of wh1ch the following 1sa specification.

This invention is an improvement in the process of hydrogenating, underhigh pressure and at an elevated temperature, natural 1 coal or otherproducts of carbonization' of wood and other vegetable matter, pitch,tar,-

wood, peat and other vegetable materials which are carbonized by theheat of the process. By such process, these carbonaceous materials aretransformed into liquids or soluble solids, or materials of lowerboilingpoint than the boiling pointof the raw materials.

In order to secure these effects according to the invention care istaken to continuously circulate the atmosphere in contact with thecarbon compound to bereacted 'on. Such circulation whereby a part of thegaseous atmosphere in contact with. the raw material is' continuouslydrawn out -of the reaction space and again returned offers anopportunity to effect the heat exchange which is' necessar to secure thereaction tem erature within the reaction vessel, and it a ordsat $5 thesame time an o portunity to separate the reaction products rom thereaction gas. .-;,;The possibility of an efiicient temperature eentrolin the. above said manner by circu- Iating the gas which is in contactwith the 40 w material broadly depends on the fact hat the gas is under'ver high press'ureof say 100 atmospheres an that therefore acomparatively smallquantity or volumev of the gas is adapted tocarryconsiderable 'quantities of heat. In order to secure the effect aimedatit is necessary to circulate a quantity of gas which is considerably inexcess of the quantity of hydrogen which is consumed by the reactionrecess. 1 In order tofacilitate t e understanding of-this invention Ihave. shown in the an-,

" nexed drawing in a diagrammatic menne'ra I suitable devicefor'efiectively carrying out my improved process.

Specification of Letters Patent. I

Patented se t. 27, 1921.

. Applteation filed April 13,1910. sum m, 92,005.

= designates the reaction vessel adapted to resist high tension. 2 is atube section forming the exit for thegaseous contents 'of the reaction,vessel. 3 is a condensing coil, 4 is a collecting vessel for condensedproducts, 5 is an absorber for ammonia with outlet 6 and inlet 7 for theabsorbing medium, 8' isa section of the circulating conduit, 9 is acirculating device, 10 is a heating coil, the exit end of which leadsinto the reaction vessel, 11 is a feeding tubefor introducingfreshreaction gas, 12 is a feeding tube for raw ma terial to be reactedon, 13 is a rotatable shaft carrying stirring members 14;.

The operation of the device is as follows.

The reaction vessel 1 is filled up to a suitable height with one of theabove mentioned raw materials or with a, mixture of suitable rawmaterials. As hydrogenating gas either hydrogen or gaseous mixturescontaming hydrogen may be used. The hydrogen or h drogen containing gasmixtures may also e formed within the rece ta'cle from substancesadapted to give 0 hydrogen under the working conditions.

The raw material is preferably introduc'ed into the reaction vessel at atemperature substantially e ual to the reactiomtemperature say 400 Thereaction gas if suitably heated within the heating coil 10 preferablyalso up to the reaction temperature of say about 400 C. reacts withinthe.

reaction vessel 1 on the raw material contained therein and is broughtin such vessel sel 4 from-which it may be drawn off at mtervals througha'oock on the vessel, The liquid drawn off from vessel 4 contains moreor 4 less of the gas'present within the reaction. vessel, nameeventually, as the-case may be, other gases.'

-The com aratively small amount of meth- 'ane, .whic deformed in theprocesamay in y hydrogen and methane and gli A this way. be removed soas to avoid its accumulation; the possibility thereof depending on thefact that methane is more soluble within liduid hydrocarbons such as areformed in this process than hydrogen. The accumulation of methane mayalso be avoided in any other suitable manner, for instance by drawingofi' either continuously or periodically more or less of the gas contained within the system and by substitutingqtherefor fresh purehydrogen.

itrogen compounds which may be contained within the raw material to betreated are under the reaction conditions in most cases transformed intoammonia which is absorbed within the absorber 5 by a suitable absorbingmedium, such as sulfuric acid. It may also be condensed to liquidammonia by coolin the gas to a temperature which is far be 0W thecondensation temperature of the hydrocarbons formed by the process andobtained within the vessel 4.

In order to be sure that the Whole of the nitrogen compounds containedin the raw material is transformed into volatile ammonia, basicsubstances, such as lime, may be added in small quantity to the rawmaterial. These basic substances neutralize the compounds of acid,character contained within the reaction material or formed during theoperation.

resh hydrogen may be introduced through pipe 11. The drawing shows asuitable device for carrying through the 'rocess only in a diagrammaticmanner. f course in practice the heat which is set freein the condensingcoil 3 may be used directly or indirectly for reheating the gas withinthe heating-coil 10. v

What I claim is 1. In-a process of hydrogenating carbon compounds underhigh pressure and at elevated temperature bringing together suitablecarbon compounds with a hydrogen containing atmosphere under suitablereaction pressure and temperature within a high pressure v'emel partlyfilled with the material to be treated, circulating the gaseous contentsof the s ace above the material under treatment, t e (}uantity ofcirculated gas being in excess 0 the consumedreac-, tion gas andsubjecting the circulated gas within the. circulating conduit to heatexchange so as to control the temperature conditions within the reactionvessel.

2. In a process of hydrogenating carbon compounds under high pressureand at ele- Tao vated temperature bringing together suitable carboncompounds with a hydrogen contaming atmosphere under suitable reactionpressure and temperature within a high pressure vessel partly filledwith-the m'aterialto be treated, circulating the gaseous contents of thespace above the material under treatment, the quantity of circul'tttedgas being in excess; of the consumed reac- 3. In a process ofhydrogenating carbon compounds under high pressure and at elevatedtemperature bringing together suitable" carbon compounds with a hydrogencontaining atmosphere under suitable reaction pressure and temperaturewithin a high pressure vessel partly filled with the material to betreated, circulating the gaseous contents of the space above thematerial under treatment, the quantity of circulated gas being in excessof the consumed reaction gas condensing the reaction product within thecirculation system, and carrying over the heat given off from the gasduring the condensation step to a section of the circulation conduitbetween the condensation section and the return point of the conduit forreheating the circulated gas.

4'. A process of hydro'genating carbon compounds consisting therein thatcarbon compounds containing nitrogen compounds are subjected to theaction of hydrogen under high pressure at elevated temperature thepresence of basic material such as ime.

V 5. A process of hydrogenati-ng solid car-' bon compounds whichconsists in heating in a retortsuch compounds in the presence'of ahydrogen atmosphere and under high reaction pressure to a high reactiontemperature, continuously abstracting a mixture of'reacs the reactionproducts, reheating the abstracted reaction gas and returning it to theretort.

tion products and reaction gas, condensing 6. A process of hydrogenatingsolid carbon compounds which consists in heating in a retort suchcompounds to a high temperature, continuously introducing hydrogen underreaction temperature and pressure,

continuously abstracting a mixture of reactionv products and freehydrogen, condensing the reaction products, reheatin the abstractedhydrogen and returning'lt to the retort.

7. A process of hydrogenating solid car-- the carbon compound,continuously. ab-

stracting a mixture of reaction products and reaction gas, condensingthe reactionprodnets, reheating the abstracted reaction gas andreturning it to the retort.

8. In a process offhydro'genating carbon compounds containingnitrogengcompounds 'underhigh pressure and at elevated temcompounds witha hydrogen'containing at- 'mosphere under suitable reaction pressure andtemperature in the resence of basic 5 material such aslime with n a highpressure vessel-partly filled with the material to be treated,circulating the gaseous contents oi the space above the material undertreatment, the quantity of circulated gas bei 1 0 in excess of,theconsumed reaction gas an subjecting the circulated gas Withinthecirculating conduit to the heat exchange so as to control thetemperature conditions within the reaction vessel. 15

9. In a process of hydrogenating carbon compounds containing nitrogencompounds under high pressure and at elevated temperature, bringingtogether suitable carbon compounds with a hydrogen containing atmosphereunder suitable reaction pressure 2! and temperature in the presence ofbasic material such as lime within a high-pressure vvessel partly filledwith the material to be treated, circulating the gaseous contents of thespace above the vmaterial under treatment, the quantity of circulatiiggas being in excess of the consumed reaction gas, con-- densing thereaction product within the circulation system, and reheating the gascooled down by the condensation process before reintroducing it into thereaction vessel.

In testimony whereof I aifix my signature in presence of two witnesses.

' DR. FRIEDRICH BERGIUS.

I Witnesses:

